EP0977731A1 - Procede de preparation d'uree - Google Patents

Procede de preparation d'uree

Info

Publication number
EP0977731A1
EP0977731A1 EP98900772A EP98900772A EP0977731A1 EP 0977731 A1 EP0977731 A1 EP 0977731A1 EP 98900772 A EP98900772 A EP 98900772A EP 98900772 A EP98900772 A EP 98900772A EP 0977731 A1 EP0977731 A1 EP 0977731A1
Authority
EP
European Patent Office
Prior art keywords
pressure
urea
melamine
reactor
ammonia
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Granted
Application number
EP98900772A
Other languages
German (de)
English (en)
Other versions
EP0977731B1 (fr
Inventor
Julius Gerardus Theodorus Van Wijck
Jozef Hubert Meessen
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Koninklijke DSM NV
DSM IP Assets BV
Original Assignee
DSM NV
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
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First worldwide family litigation filed litigation Critical https://patents.darts-ip.com/?family=19764295&utm_source=google_patent&utm_medium=platform_link&utm_campaign=public_patent_search&patent=EP0977731(A1) "Global patent litigation dataset” by Darts-ip is licensed under a Creative Commons Attribution 4.0 International License.
Application filed by DSM NV filed Critical DSM NV
Publication of EP0977731A1 publication Critical patent/EP0977731A1/fr
Application granted granted Critical
Publication of EP0977731B1 publication Critical patent/EP0977731B1/fr
Anticipated expiration legal-status Critical
Expired - Lifetime legal-status Critical Current

Links

Classifications

    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C273/00—Preparation of urea or its derivatives, i.e. compounds containing any of the groups, the nitrogen atoms not being part of nitro or nitroso groups
    • C07C273/02—Preparation of urea or its derivatives, i.e. compounds containing any of the groups, the nitrogen atoms not being part of nitro or nitroso groups of urea, its salts, complexes or addition compounds
    • C07C273/12—Preparation of urea or its derivatives, i.e. compounds containing any of the groups, the nitrogen atoms not being part of nitro or nitroso groups of urea, its salts, complexes or addition compounds combined with the synthesis of melamine

Definitions

  • the invention relates to a process for preparing urea, in which the gas stream which is released during the synthesis of melamine and is essentially composed of ammonia and carbon dioxide is used for the synthesis of urea.
  • a preparation of urea in which the offgas which is essentially composed of ammonia and carbon dioxide and is obtained in the preparation of melamine in a high-pressure melamine process is used for the synthesis of urea.
  • the gas stream from the gas/liquid separator of the melamine plant which is essentially composed of ammonia and carbon dioxide, is transferred to a low-pressure section of a conventional high- pressure urea plant.
  • the ammonia and carbon dioxide originating from the melamine plant are reacted in an additional reactor to form a urea solution.
  • Said urea solution is then increased in pressure and transferred to the high- pressure section of the same urea plant.
  • Urea can be prepared by passing ammonia and carbon dioxide at a suitable pressure (for example, 12.5 - 35 MPa) and a suitable temperature (for example, 160 - 250 °C) into a synthesis zone in which ammonium carbamate is first formed according to the reaction
  • urea is then formed by dehydration according to the equilibrium reaction: H 2 N-CO-ONH 4 ⁇ * * H 2 N-CO-NH 2 + H 2 0
  • the extent to which this conversion proceeds is dependent, inter alia, on the temperature and the excess of ammonia used.
  • a solution which is composed essentially of urea, water, ammonium carbamate and unreacted ammonia is obtained as the reaction product.
  • the ammonium carbamate and the unreacted ammonia have to be removed from the solution and are in most cases fed back to the synthesis zone.
  • the synthesis zone may comprise separate zones for the formation of ammonium carbamate and urea. However, these zones may also be combined in one apparatus.
  • a conventional high-pressure urea plant is understood to be a urea plant in which the decomposition of the ammonium carbamate not converted into urea and the expulsion of the usual excess of ammonia takes place at a substantially lower pressure than the pressure in the synthesis reactor itself.
  • the synthesis reactor is usually operated at a temperature of 180 - 210°C and a pressure of 18 - 30 MPa.
  • the unreacted reactants are fed back, after expansion, dissociation and condensation, at a pressure of between 1.5 and 10 MPa to the urea synthesis.
  • ammonia and carbon dioxide are fed directly to the urea reactor.
  • the object of the invention is to find a process which does not have these disadvantages .
  • a urea stripping plant is understood to be a urea plant in which the decomposition of the ammonium carbamate not converted into urea and the expulsion of the normal excess of ammonia take place mostly at a pressure which is essentially almost equal to the pressure in the synthesis reactor. This decomposition/ expulsion takes place in a stripper, optionally with the addition of a stripping medium.
  • carbon dioxide and/or ammonia can be used as stripping medium before said components are metered to the reactor.
  • Said stripping takes place in a stripper placed downstream of the reactor in which the solution which originates from the urea reactor and which contains, in addition to urea, ammonium carbamate, water, ammonia and carbon dioxide, is stripped with heat being fed. It is also possible to use thermal stripping here. Thermal stripping means that ammonium carbamate is decomposed and the ammonia and carbon dioxide present are removed from the urea solution exclusively by means of supplying heat. The streams which are released from the stripper and contain ammonia and carbon dioxide are fed back via a high- pressure carbamate condenser to the reactor. The reactor, the stripper and the high-pressure carbamate condenser form the most important components of the high-pressure section of a urea stripping plant.
  • the synthesis reactor is preferably operated at a temperature of 160 - 220°C and a pressure of 12.5 - 17.5 MPa.
  • the N/C ratio in the synthesis is between 2.5 and 4.
  • the substantially anhydrous carbamate stream from the condenser from the high-pressure melamine process is fed to a high-pressure section of a urea stripper plant and can be fed, for example, to a urea reactor, to a stripper, to a high-pressure carbamate condenser or to lines present between these.
  • the substan-tially anhydrous carbamate from the condenser of the high-pressure melamine process is fed directly to the urea reactor.
  • the condensation can be carried out in a condenser which is operated at a pressure which is substantially equal to the pressure in the melamine reactor.
  • the condenser is designed as a heat exchanger.
  • a coolant is fed to the jacket side and the gas stream composed of carbon dioxide and ammonia is fed through the tube bundle. It is also possible to feed the gas stream through the jacket and the coolant through the tube bundle. Since the condensation temperature in said condenser is between 100 and 230°C, vaporizing boiler feed water can be used as coolant, which has the additional advantage that the heat of condensation can profitably be used to produce low-pressure steam (0.3 to 1.0 MPa). If no profitable use is present in the plant surroundings for said low-pressure steam, cooling water can also, of course, be used as coolant.
  • the advantage of the use of a carbamate stream from the high-pressure melamine plant is that a substantially anhydrous carbamate stream is obtained for the urea stripper plant which, as a result of its substantially anhydrous nature, ensures an improved efficiency in the urea plant compared with a urea plant which obtains a water-containing carbamate stream from the melamine plant.
  • An additional advantage can be obtained by feeding the substantially anhydrous carbamate stream directly to the urea reactor.
  • the pressure of the carbamate flow originating from the condenser of the high-pressure melamine plant is between 5 and 80 MPa, preferably between 8 and 40 MPa.
  • the pressure of the carbamate stream originating from the high-pressure melamine plant is 0-10 MPa and, more particularly, 0-2 MPa higher than the pressure in the urea reactor.
  • the temperature of said carbamate stream is between 100 and 230°C, preferably between 140 and 200°C.
  • the high-pressure carbamate condenser can, for example, be designed as a so-called flooded condenser as described in NL-A-8400839.
  • the gas mixture to be condensed is fed into the jacket space of a tube exchanger, into which jacket space a dilute carbamate solution is also fed, and the heat of solution and condensation released is removed with the aid of a medium flowing through tubes, for example water, which is converted in this process into low- pressure steam.
  • the flooded condenser may be arranged horizontally or vertically. However, particular advantages are offered by carrying out the condensation in a horizontally arranged flooded condenser (a so- called pool condenser; see, for example, Nitrogen No.
  • the said urea reactor comprises a horizontally arranged condensation zone and a heat exchanger (a so-called pool reactor; see, for example, Nitrogen No. 222, July-August 1996, pages 29- 31) in which ammonia and carbon dioxide are fed to the reactor and largely adsorbed in the urea synthesis solution. A substantial part of the heat produced by the condensation is removed with the aid of the heat exchanger.
  • the residence time of the urea synthesis solution in the reactor is chosen so that at least 85% of the theoretically obtainable quantity of urea is prepared, after which the urea synthesis solution is processed to form a urea solution or solid urea.
  • the stripped urea synthesis solution is let down to a low pressure and evaporated, and the urea melt obtained in this process is completely or partly transferred to the melamine plant .
  • the preparation of melamine preferably starts from urea as raw material, preferably in the form of a melt .
  • Ammonia and carbon dioxide are by-products during the melamine preparation, which proceeds according to the following reaction equation:
  • the preparation can be carried out at a pressure of between 5 and 80 MPa without the presence of a catalyst.
  • the temperature of the reaction is between 300 and 500°C and is preferably between 350 and 425°C.
  • a device for the preparation of melamine which is suitable for the present invention may comprise, for example, a melamine scrubber, a reactor, optionally combined with a gas-liquid separator or having a separate gas-liquid separator, optionally an afterreactor or ageing vessel placed downstream of the reactor, and a product cooler/product working-up section.
  • Placed downstream of the melamine scrubber is a condenser for converting the gas stream originating from the melamine scrubber into substantially anhydrous ammonium carbamate .
  • melamine is produced from urea in a device comprising, for example, a condenser, a melamine scrubber, a reactor for the production of melamine, optionally an afterreactor or ageing vessel and a product cooler.
  • urea melt is fed from the urea plant to a melamine scrubber at a pressure of 5-80 MPa, preferably 8-40 MPa, and at a temperature above the melting point of urea.
  • Said melamine scrubber can be provided with a jacket in order to provide additional cooling in the scrubber.
  • the melamine scrubber may also be provided with internal cooling bodies.
  • the liquid urea comes into contact with reaction gases from the melamine reactor or from a separate separator placed downstream of the reactor.
  • the reaction gases are composed essentially of carbon dioxide and ammonia and also contain a quantity of melamine vapour.
  • the molten urea scrubs the melamine vapour out of the offgas and carries said melamine back to the reactor.
  • the offgases composed essentially of ammonia and carbon dioxide are removed from the top of the melamine scrubber, converted into ammonium carbamate in a condenser and returned to the high-pressure section of a urea plant, in which urea is produced by means of the stripping process, in order to be used therein as a raw material for urea production.
  • the pressure of said carbamate stream is almost equal to the pressure in the melamine reactor and is between 5 and 80 MPa, preferably between 8 and 40 MPa. More particularly, the pressure is 0-10 Mpa higher than the pressure in the urea reactor and still more particularly 0-2 MPa higher than the pressure in the urea reactor.
  • the temperature of said carbamate stream is preferably between 140 and 200°C.
  • the preheated urea is removed from the melamine scrubber and fed, together with the scrubbed melamine, by means of, for example, a high-pressure pump to the reactor, which is at a pressure of 5 to 80 MPa and preferably of 8 to 40 MPa.
  • a high-pressure pump to the reactor, which is at a pressure of 5 to 80 MPa and preferably of 8 to 40 MPa.
  • use can also be made of gravity by placing the melamine scrubber above the reactor.
  • the molten urea is heated to a temperature of 300 to 500°C, preferably of approximately 350 to 425°C, at a pressure of 5 to 80 MPa, preferably of 8 to 40 MPa, under which conditions the urea is converted into melamine, carbon dioxide and ammonia .
  • a quantity of ammonia can be metered to the reactor.
  • the ammonia added may serve, for example, as a purging agent for preventing blockage of the reactor bottom or to avoid the formation of condensation products of melamine, such as melam, melem and melon or to promote the mixing in the reactor.
  • the quantity of ammonia fed to the reactor is 0-10 mol per mole of urea, preferably 0-5 mol is used and in particular 0-2 mol of ammonia per mole of urea.
  • the carbon dioxide and ammonia produced in the reaction, and also the ammonia additionally fed, collect in the separation section, for example in the top of the reactor, but a separate separator placed downstream of the reactor is also possible, and are separated in the gaseous state from the liquid melamine.
  • the gas mixture produced is passed to the melamine scrubber to remove melamine vapour and to preheat the urea melt .
  • the liquid melamine is removed from the reactor and, in this embodiment, is transferred, for example, to an afterreactor, but transfer directly to the product cooler is also possible.
  • the liquid melamine is brought into contact with 0. Olio mol of ammonia per mole of melamine and, preferably, 0.1-2 mol of ammonia per mole of melamine.
  • the contact time in the afterreactor or in the ageing vessel is between 1 minute and 10 hours.
  • the temperature and the pressure in the afterreactor or ageing vessel are almost the same as in the reactor in which urea is converted into melamine.
  • the liquid melamine present in the afterreactor or ageing vessel is removed from the afterreactor or ageing vessel and transferred to a product cooler. In the product cooler, the liquid melamine is cooled by bringing it into contact with a coolant.
  • a coolant Preferably ammonia, and in particular liquid ammonia, is chosen as the coolant.
  • the melamine is converted into powdered form and is removed from the cooling unit via the bottom of the product cooler.
  • an evaporation step is included between the reactor or, possibly, the afterreactor and the product cooler.
  • liquid melamine is converted into gaseous melamine, in which process the by-products, such as, for example, melam, remain behind in the evaporator.
  • process the by-products such as, for example, melam
  • the advantage of this is that the amount of by-products in the melamine is reduced. In this way, melamine having a very high degree of purity is obtained. It is also possible to meter in additional ammonia during the evaporation. According to this process, gaseous melamine is then cooled with ammonia in the product cooler.
  • Example 1 The invention is explained in greater detail by reference to the following examples .
  • Example 1 Example 1 :
  • a gas stream of 53.6 kg/hour is transferred from the melamine scrubber to a condenser.
  • the pressure of said gas stream is 8 MPa and the temperature is 186°C.
  • the composition is as follows: 50.3 wt . % ammonia, 49.3 wt . % carbon dioxide, 0.2 wt.% water, 0.2 wt . % urea .
  • the pressure in the condenser is maintained at almost 8 MPa and the temperature is lowered. At a temperature of 144°C, almost complete condensation of the gas stream occurs.
  • the liquid mixture produced is transferred by a pump to the high-pressure section of a urea synthesis.
  • a gas stream of 60 kg/hour is transferred from the melamine scrubber to a condenser.
  • the pressure of said gas stream is 15 MPa and the temperature is 202°C.
  • the composition is as follows: 50.3 wt . % ammonia, 49.2 wt.% carbon dioxide, 0.3 wt.% water, 0.2 wt.% urea.
  • the pressure in the condenser is maintained at virtually 15 MPa and the temperature is lowered. At a temperature of 166°C, almost complete condensation of the gas stream occurs .
  • the liquid mixture produced is transferred directly to the high-pressure section of a urea synthesis and is fed there to the inlet of the high-pressure carbamate condenser.
  • Example 3 A gas stream of 51.2 kg/hour is transferred from the melamine scrubber to a condenser. The pressure of said gas stream is 20 MPa and the temperature 207°C. The composition is as follows: 50.4 wt . % ammonia, 49.2 wt . % carbon dioxide, 0.2 wt.% water, 0.2 wt . % urea .
  • the pressure in the condenser is maintained at almost 20 MPa and the temperature is lowered. At a temperature of 175°C, almost complete condensation of the gas stream occurs while at the same time steam of 0.3 MPa is generated.
  • the liquid mixture produced is transferred directly to the high-pressure section of a urea synthesis and is fed there to the feed line of the urea reactor.

Landscapes

  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
  • Agricultural Chemicals And Associated Chemicals (AREA)
EP98900772A 1997-01-29 1998-01-20 Procede de preparation d'uree Expired - Lifetime EP0977731B1 (fr)

Applications Claiming Priority (3)

Application Number Priority Date Filing Date Title
NL1005118 1997-01-29
NL1005118A NL1005118C2 (nl) 1997-01-29 1997-01-29 Werkwijze voor de bereiding van ureum.
PCT/NL1998/000036 WO1998032731A1 (fr) 1997-01-29 1998-01-20 Procede de preparation d'uree

Publications (2)

Publication Number Publication Date
EP0977731A1 true EP0977731A1 (fr) 2000-02-09
EP0977731B1 EP0977731B1 (fr) 2002-07-10

Family

ID=19764295

Family Applications (1)

Application Number Title Priority Date Filing Date
EP98900772A Expired - Lifetime EP0977731B1 (fr) 1997-01-29 1998-01-20 Procede de preparation d'uree

Country Status (16)

Country Link
US (1) US6111138A (fr)
EP (1) EP0977731B1 (fr)
JP (1) JP4063333B2 (fr)
KR (1) KR100522226B1 (fr)
CN (1) CN1119326C (fr)
AT (1) ATE220392T1 (fr)
AU (1) AU726205B2 (fr)
CA (1) CA2279235C (fr)
DE (1) DE69806475T2 (fr)
ES (1) ES2180139T3 (fr)
ID (1) ID22135A (fr)
NL (1) NL1005118C2 (fr)
NO (1) NO312545B1 (fr)
PL (1) PL196634B1 (fr)
TW (1) TW513396B (fr)
WO (1) WO1998032731A1 (fr)

Families Citing this family (30)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US6380385B1 (en) 1995-12-07 2002-04-30 Agrolinz Melanin Gmbh Process for the preparation of pure melamine
AT411830B (de) * 1998-12-03 2004-06-25 Agrolinz Melamin Gmbh Verfahren zur herstellung von harnstoff unter einbindung der melamin-offgase in eine harnstoffanlage
NL1014280C2 (nl) * 2000-02-03 2001-08-06 Dsm Nv Werkwijze voor de bereiding van melamine uit ureum.
NL1021637C2 (nl) * 2002-07-29 2004-01-30 Dsm Nv Werkwijze voor het vergroten van de capaciteit van een ureumfabriek.
US7597675B2 (en) 2004-12-22 2009-10-06 össur hf Knee brace and method for securing the same
US7713225B2 (en) 2004-12-22 2010-05-11 Ossur Hf Knee brace and method for securing the same
US8425441B2 (en) * 2004-12-22 2013-04-23 Ossur Hf Spacer element for use in an orthopedic or prosthetic device
US8585623B2 (en) * 2004-12-22 2013-11-19 Ossur Hf Orthopedic device
US8231560B2 (en) * 2004-12-22 2012-07-31 Ossur Hf Orthotic device and method for securing the same
US8216170B2 (en) 2004-12-22 2012-07-10 Ossur Hf Orthopedic device
US7794418B2 (en) * 2004-12-22 2010-09-14 Ossur Hf Knee brace and method for securing the same
DE602005024680D1 (de) * 2005-08-10 2010-12-23 Urea Casale Sa Verfahren zur integrierten Herstellung von Harnstoff und Melamin
US7687041B2 (en) * 2008-02-27 2010-03-30 Kellogg Brown & Root Llc Apparatus and methods for urea production
EP2439191B1 (fr) * 2009-08-21 2017-01-25 Asahi Kasei Kabushiki Kaisha Procédé pour la production d'ester d'acide carbamique n-substitué, procédé pour la production d'isocyanate à l'aide d'ester d'acide carbamique n-substitué et composition pour le transfert et le stockage d'ester d'acide carbamique n-substitué contenant de l'ester d'acide carbamique n-substitué et un composé hydroxy aromatique
KR101389545B1 (ko) 2012-04-27 2014-05-30 제우스산업 주식회사 암모니아 가스를 재사용하여 글리세롤로부터 글리세롤 카보네이트를 제조하는 방법
US9474334B2 (en) 2012-11-13 2016-10-25 Ossur Hf Fastener member for affixation to a structure in an orthopedic device and method for securing the same
WO2014107697A2 (fr) 2013-01-07 2014-07-10 Ossur Hf Dispositif orthopédique et son procédé de fixation
EP2950759B1 (fr) 2013-01-31 2020-05-13 Ossur Hf Dispositif orthopédique ayant des composants détachables pour des stades de traitement
EP2950758B1 (fr) 2013-01-31 2020-11-18 Össur HF Ensemble sangle de force progressive destiné à être utilisé avec un dispositif orthopédique
WO2014168910A1 (fr) 2013-04-08 2014-10-16 Ossur Hf Système de fixation de bande pour dispositif orthopédique
US10052221B2 (en) 2015-01-06 2018-08-21 Ossur Iceland Ehf Orthopedic device for treating osteoarthritis of the knee
EP3463215B1 (fr) 2016-06-06 2022-02-16 Ossur Iceland EHF Dispositif orthopédique
US11850175B2 (en) 2016-06-06 2023-12-26 Ossur Iceland Ehf Orthopedic device, strap system and method for securing the same
US11712359B2 (en) 2017-10-06 2023-08-01 Ossur Iceland Ehf Connector for an orthopedic device
IT201800006795A1 (it) * 2018-06-29 2019-12-29 Procedimento di conversione diretta di off-gas anidri da impianti melammina in urea
USD888258S1 (en) 2018-10-08 2020-06-23 Ossur Iceland Ehf Connector assembly
USD882803S1 (en) 2018-10-08 2020-04-28 Ossur Iceland Ehf Orthopedic shell
USD908458S1 (en) 2018-10-08 2021-01-26 Ossur Iceland Ehf Hinge cover
WO2022146806A1 (fr) 2020-12-28 2022-07-07 Ossur Iceland Ehf Manchon et procédé d'utilisation avec dispositif orthopédique
WO2024112198A1 (fr) 2022-11-22 2024-05-30 Stamicarbon B.V. Installation de production de mélamine/urée avec condenseur gaz de dégagement de mélamine

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DE1770969C3 (de) * 1968-07-25 1978-08-24 Basf Ag, 6700 Ludwigshafen Verfahren zur Rückführung der Abgase der Melaminsynthese in die Hamstoffsynthese
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US3723430A (en) * 1970-10-28 1973-03-27 Nissan Chemical Ind Ltd Method for reclamation of melamine waste gas
US4433146A (en) * 1982-04-07 1984-02-21 Stamicarbon B.V. Process for the preparation of melamine
NL8400839A (nl) * 1984-03-16 1985-10-16 Unie Van Kunstmestfab Bv Werkwijze voor de bereiding van ureum.

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Also Published As

Publication number Publication date
PL334875A1 (en) 2000-03-27
EP0977731B1 (fr) 2002-07-10
NO312545B1 (no) 2002-05-27
US6111138A (en) 2000-08-29
WO1998032731A1 (fr) 1998-07-30
NO993698D0 (no) 1999-07-29
CN1251088A (zh) 2000-04-19
KR20000070500A (ko) 2000-11-25
ES2180139T3 (es) 2003-02-01
AU5578898A (en) 1998-08-18
NL1005118C2 (nl) 1998-07-30
DE69806475T2 (de) 2003-02-27
CA2279235A1 (fr) 1998-07-30
TW513396B (en) 2002-12-11
JP4063333B2 (ja) 2008-03-19
AU726205B2 (en) 2000-11-02
CA2279235C (fr) 2006-12-12
ATE220392T1 (de) 2002-07-15
JP2001509159A (ja) 2001-07-10
CN1119326C (zh) 2003-08-27
NO993698L (no) 1999-09-21
PL196634B1 (pl) 2008-01-31
KR100522226B1 (ko) 2005-10-17
DE69806475D1 (de) 2002-08-14
ID22135A (id) 1999-09-09

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